Bayer CropScience AG Page 1 of 82 BCS-RD-D ... - IR-4 Project

More documents

Recommendations

Info

Bayer CropScience AG Page 10 of 82 BCS-RD-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 1 Summary (contd) The stability of BYI08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc) in diluted plant extracts in acetonitrile/water was determined at the respective LOQ levels. The extracts of three untreated control samples were separately fortified with each analyte and after initial analysis, these solutions were stored in a refrigerator and re-analysed after 2, 5, 8 and 16 days. The diluted extracts of treated samples were stored under the same conditions as control extracts (in a refrigerator at 4°C ± 3°C). The results indicate that all analytes are stable in plant extracts for at least two weeks. The recovery serves as a measure of the accuracy of the analytical method. The individual recovery rates for BYI08330 ranged from 72 to 108% with overall means (n = 6 - 10) between 87 and 101% and overall RSDs of up to 13.3%. The individual recovery rates for BYI08330-enol ranged from 69 to 111% with overall means (n = 6 - 10) between 86 and 104% and overall RSDs of up to 15.0%. The individual recovery rates for BYI08330-mono-hydroxy ranged from 68 to 110% with overall means (n = 6 - 10) between 88 and 101% and overall RSDs of up to 13.7%. The individual recovery rates for BYI08330-ketohydroxy ranged from 69 to 111% with overall means (n = 6 - 10) between 87 and 101% and overall RSDs of up to 14.6%. The individual recovery rates for BYI08330-enol-Glc ranged from 70 to 109% with overall means (n = 6 - 10) between 86 and 98% and overall RSDs of up to 15.1%. As a measure for the precision of the method, the intra-laboratory repeatability (n = 5) is given as relative standard deviation (% RSD) for different sample materials (e.g. orange fruit, plum fruit, apple fruit, apple sauce, potato tuber, hop beer) at fortification levels of 0.01 and 0.1 mg/kg or 1.0 and 10 mg/kg (only hop cone dried and green). The RSD of the repeatability tests at each recovery set ranged from 0.5 to 14.0%. The validation data obtained demonstrate the high sensitivity, selectivity, accuracy and precision (repeatability) of the method for determination of BYI08330 (parent compound, total residue of) and its metabolites BYI08330-enol, BYI08330-mono-hydroxy, BYI08330-ketohydroxy and BYI08330-enol-Glc in plant material. For confirmation of the results a second MRM transition was recorded for each individual analyte and each investigated matrix.
Bayer CropScience AG Page 11 of 82 BCS-RD-D-ROCS Method-No. 00857 D-40789 Monheim Report No. MR-099/04 2 Introduction The analytical method 00857 presented in this report was developed in order to determine residues of BYI08330 (parent compound, total residue of BYI08330) and its metabolites BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in/on plant material by HPLC-ESI-MS/MS using stable isotopically labelled internal standards. 2.1 BYI08330 Active Ingredient: BYI08330 Chemical Name: cis-3-(2,5-dimethylphenyl)-8-methoxy-2-oxo-1-azaspiro[4,5]dec-3-en-4-yl ethyl carbonate Empirical Formula: C21H27NO5 Molecular Mass: Structural Formula: 373.45 g/mol H3C O O H O CH3 2.2 BYI08330-enol Empirical Formula: C18H23NO3 Molecular Mass: 301.39 g/mol Structural Formula: CH 3 CH 3 HO CH3 CH 3 O O O NH NH H O CH 3
Page 1 and 2: Bayer CropScience AG Page 1 of 82 B
Page 12 and 13: Bayer CropScience AG Page 12 of 82
Page 60 and 61:
Bayer CropScience AG Page 60 of 82
Page 62 and 63:
Page 64 and 65:
Page 66 and 67:
Page 68 and 69:
Page 70 and 71:
Page 72 and 73:
Page 74 and 75:
Page 76 and 77:
Page 78 and 79:
Page 80 and 81:
Page 82:
show all

Bayer CropScience AG Page 1 of 82 BCS-RD-D ... - IR-4 Project

You also want an ePaper? Increase the reach of your titles

Delete template?

Save as template?